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Method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing industrial chromatography technology

A technology of dihydroflavonoid glycosides and industrial chromatography, which is applied in the field of separation and purification of active ingredients of traditional Chinese medicine, can solve the problems that the separation process cannot realize real-time online monitoring, the purity and yield of ingredients are not high, and the purity of active ingredients is not high, so as to improve the quality of medicinal materials. The effect of utilization rate, short preparation process and simple operation

Pending Publication Date: 2021-07-16
JIANGZI QINGFENG PHARMACEUTICALS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, either the purity of the active ingredients prepared by these processes is not high, it is a mixture of various substances, and thorough separation and purification have not been achieved; either the purity and yield of various components are not high; or the separation and purification process is difficult to industrialize Small batch production, and the separation process cannot realize real-time online monitoring, the separation process is blind, and the sensitivity is low

Method used

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  • Method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing industrial chromatography technology
  • Method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing industrial chromatography technology
  • Method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing industrial chromatography technology

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Take Citrus aurantium, cut into decoction pieces or crush, add 4 times the amount of water, decoct 3 times, decoct and extract for 3 hours each time, combine the decoction liquid, filter, the filtrate passes through the treated non-polar macroporous resin, and then Elute with water and ethanol below 20% (19%) to remove impurities, then elute with 25% ethanol and 2% sodium hydroxide, collect the 25% ethanol eluate, concentrate under reduced pressure at 50-70°C to a relative density of about 1.40 The fluid extract, dried under reduced pressure at 80°C, and pulverized to obtain the total flavonoids extract of Citrus aurantium (see its HPLC chromatogram figure 1 ).

Embodiment 2

[0035] Take the citrus aurantium, cut into decoction pieces or crush, add 15 times the amount of water, decoct once, extract for 1 hour each time, combine the decoction liquid, filter, the filtrate passes through the treated non-polar macroporous resin, and then Elute with water and ethanol (15%) below 20% to remove impurities, then elute with 90% ethanol and 0.5% sodium hydroxide, collect the 90% ethanol eluate, concentrate under reduced pressure at 50-70°C to a relative density of about 1.20 The liquid extract was dried under reduced pressure at 60°C and crushed to obtain the total flavonoids extract of Citrus aurantium.

Embodiment 3

[0037] A kind of method that utilizes industrial chromatographic technique to prepare two kinds of dihydroflavonoid glycoside monomer compounds simultaneously (technical process sees figure 2 ), the dihydroflavone glycoside monomer compound is naringin and neohesperidin, comprising the following steps:

[0038] Get the total flavonoid glycosides extract of Fructus Fructus Fructus Aurantii gained in Example 1 (its HPLC chromatogram sees figure 1), wherein the content of naringin is about 15.0% (W / W), and the content of neohesperidin is about 20.0% (W / W), adding 5.0% (V / V) ethanol aqueous solution to dissolve it and prepare 105mg / ml concentration solution, filtered to obtain the sample solution.

[0039] Inject 100L of the sample solution into the industrial dynamic axial compression column system, the industrial chromatographic filler is UniSil30-100 (C18), ethanol: water: trifluoroacetic acid solution (35:65:0.3, V / V / V) as the eluent , the elution flow rate is 10.0CV / h, th...

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Abstract

The invention discloses a method for simultaneously preparing two flavanone glycoside monomeric compounds by utilizing an industrial chromatography technology, the flavanone glycoside monomeric compounds are naringin and neohesperidin, and the purities of the naringin and the neohesperidin are both above 99.5%. The method provided by the invention can realize real-time online monitoring of the separation process, which has good process reproducibility, simple operation, short preparation process, low organic solvent consumption, economical and environment-friendly, high economic benefit and can be used for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, in particular to a method for simultaneously preparing two dihydroflavone glycoside monomers by using industrial chromatography technology, specifically a method for simultaneously preparing naringin by using an industrial dynamic axial compression column system and the method of neohesperidin. Background technique [0002] Citrus aurantium is the dried young fruit of Citrus aurantium L. and its cultivars of the Rutaceae plant or sweet orange Citrussinensis Osbeck. , Severe dysentery after diarrhea, obstructed stool, phlegm stagnation and air obstruction, chest obstruction, chest knot, gastroptosis, prolapse of the anus, uterine prolapse and other diseases. According to literature reports, Citrus aurantium mainly contains flavonoids, alkaloids, volatile oils, coumarins and other components. In terms of pharmacological ef...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCC07H17/07C07H1/08
Inventor 周鹏王章伟刘地发刘玉华张功俊古福生梁佳王振谢标鹏魏勇翔张九月
Owner JIANGZI QINGFENG PHARMACEUTICALS INC
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